Diisopropylethylamine → (E)-3-Cyclopropyl-N-[2-[(2-m ethoxy-6-methyl-pyrimidin-4-yl)-methyl-amino]ethyl]prop-2-enamide
反応式
[CH:1]1(/[CH:4]=[CH:5]/[C:6]([OH:8])=O)[CH2:3][CH2:2]1.C(N(C(C)C)CC)(C)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:42][O:43][C:44]1[N:49]=[C:48]([N:50]([CH3:54])[CH2:51][CH2:52][NH2:53])[CH:47]=[C:46]([CH3:55])[N:45]=1>CN(C=O)C>[CH:1]1(/[CH:4]=[CH:5]/[C:6]([NH:53][CH2:52][CH2:51][N:50]([C:48]2[CH:47]=[C:46]([CH3:55])[N:45]=[C:44]([O:43][CH3:42])[N:49]=2)[CH3:54])=[O:8])[CH2:2][CH2:3]1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
(E)-3-Cyclopropylprop-2-enoic acid (11.2 mg, 0.1 mmol) and diisopropylethylamine (17.4 μl, 1 mmol) were dissolved in anhydrous DMF (0.5 ml), HBTU (39 mg, 0.1 mmol) was added and the mixture was stirred for 15 minutes at room temperature. N-(2-methoxy-6-methyl-pyrimidin-4-yl)-N-methyl-ethane-1,2-diamine (19.6 mg, 0.1 mmol) and diisopropylethylamine (17.4 μl, 0.1 mmol), dissolved in anhydrous DMF (0.5 ml) were added and the mixture was stirred at room temperature overnight. The mixture was purified directly by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile) to yield 13.7 mg (0.047 mmol, 47.2%).
後処理
- additionwere added
- stirringthe mixture was stirred at room temperature overnight
- customThe mixture was purified directly by preparative HPLC (gradient of water containing 0.1% NH3 and acetonitrile)
- customto yield 13.7 mg (0.047 mmol, 47.2%)
出典と根拠
- ORDレコード
- ord-9df32414948c47039c2484dfb955b4ba
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877934B2
反応ノート
読み込み中…